IS : 79-lS7C ( Reaffirmed 2004 ) Indian Standard SPECIFICATION FOR LINSEED STAND OIL FOR PAINTS ( First Revision 1 First Reprint DECEMBER 1995 UDC 667.621~52 ; 6651345.4 BUREAU MANAK OF BHAVAN, INDIAN STANDARDS WFAR MARC3 9 BAHADUR SHAH NBW DELHI 110002 Gr 4 May 1976 IS : 79 - 1975 Indian Standard SPECIFICATION FOR LINSEED STAND OIL FOR PAINTS (First Revision) Raw Materials for Paint [ndustry Sectional Committee, CDC 50 Chairman DR R. J. RATHI Representing Sudarshan Chemical Industries Ltd, Pune K. L. RATHI (Alternate to Dr R. J. Rathi) SHRI S. K. ASTHANA SHRI S. PANDEY (Al&ma&) SHRI C. J. BHUMKAR SHRI G. C. DESAI SHRI S. H. DESAI SHRI R. R. SEQUEIRA(Al&emu&) SHRI G. S. GILL DR P. K. BHANDARI (Alternate) JOINT DIRECTOR (M & C) AWSTANT RESEARCH OFFICER (CHEM)-I (Alternate) SHRI K. V. KRISHNAN SHRI R. M. TILLU (Alternate) SURI T. K. S. MANI SHRI Ministry of Defence (DGI) Asian Paints (India) Ltd, Bombay Goodlass Nerolac Paints Ltd, Bombay Blundell Eomite Paints Ltd, Bombay Indian Paint Association, Calcutta Railway Board (Ministry of Railways) Colour-Chem Ltd, Bombay Addisons Paints & Chemicals. Ltd, Madras; and Paints & Allied Products Sectional Committee, CDC 8, ISI SHRI M. B. SATYANARAYANA (Alternate) Chowgule & Co (Hind) Pvt Ltd, Bombay SHRI V. M. NACHANE Travancore Titanium Products Ltd, Trivandrum DR V. S. VIHAYAN NAYAR Kamani Metallic Oxides Pvt Ltd, Bombay SHRI V. C. PANCHAMIYA Ministry of Defence (R & D) DR B. SANYAL SHRI K. K. CHOUDHRY(Alternate) The Development Commissioner, Small Scale SHRI P. SATYANARAYANAN Industries, New Delhi National Test House, Calcutta SHRI K. C. SEAL Directorate General of Technical Development, SHRI K. N. R. SHARMA New Delhi SHRI KUI.TAR SINCH (Al&mate) (Continued on page 2) (Q Copyright 1976 BUREAU OF INDIAN STANDARDS This publication is protected under the Indian Copyright Act (XIV of 1957) and reproduction in whole or in part by any means except with written permission of the publisher shall be deemed to be an infringement of copyright under the said Act. , IS : 79 - 1975 (Continued from page 1) Members SHUNCLU Rqhcscnting State Trading Corporation of India Ltd, New Delhi The Alkali and Chemical Corporation of India Ltd, Calcutta (Alternate) Hindustan Petroleum Corporation Ltd, Bombay Director General, ISI (&o&o Member) Secretary SHRI R. K. SINOH SHRI P.K. The SHRI Y. S. SWAMY SHRI S. BHATTACHARYA SHRI K. S. THAKKAR DR G. M. SAXENA, Director (Chem) Assistant Director (Chem), ISI Drying Oils Subcommittee, Asian Paints CDC 50 : 2 (India) Ltd, Bombay conocw SHRI R. B. GOYAL Members SHRI SUKESH BOSE SHRI S. H. DESAI SHRI S. L. GARC SHRI S. K. GARO (Alternate) SHRI G. K. GHOSH SHRI N. K. SWAIICA (Ah-mate) DR S. N. MODAK DR I. G. THAPER (Alternate) SHRI V. M. NACHANE DR M. A. SIVA~AMBAN British Paints (India) Ltd, Calcutta Blundell Eomite Paints Ltd, Bombay Technic0 Enterprises Pvt Ltd, Calcutta Swaika Oil Mills, Calcutta Oil Industries Pvt Ltd, Bombay The Bombay Chowgule & Co (Hind) Pvt Ltd, Bombay Regional Research Laboratory (CSIR), Hyderabad Ad-hoc COIWW Panel of Calcutta National Regidn, Test House, CDC 50: P2 DR A. S. BHADIJRI Calcutta Members DR P. K. BHANDARI SHRI M. M. GH~SE SHRI G. K. GHOSH SHRI M. N. RAO SHRI S. K. ROY SHRJ G. N. TIWARI Indian Paint Association, Calcutta Shalimar Paints Ltd, Calcutta Swaika Oil Mills Ltd, Calcutta British Paints (India) Ltd, Calcutta Allied Resins & Chemicals Pvt Ltd, Caktttta The Alkali and Chemical Corporation of India Ltd, Calcutta 2 ls I 79-1975 Indian Standard SPECIFICATION FOR LINSEED STAND OIL FOR PAINTS (First Revision) 0. FOREWORD 0.1 This Indian Standard (First Revision) was adopted by the Indian Standards Institution on 15 December 1975, after the draft finalized by the Raw Materials for Paint Industry Sectional Committee had been approved by the Chemical Division Council. 0.2 This standard was first published in 1950 and was based largely on the interim coordinated draft produced with the assistance of the representatives of manufacturers and various departments and authorities of the Government of India, by the Coordinating Subcommittee of the No. 5 Standing Committee on Specifications for Paints and Allied Stores of the General Headquarters (now Army Headquarters), India. 0.3 In this revision, substantial alignment with ISO/R 276 `Linseed stand oil' issued by the Int.ernational Organization for Standardization (ISO), has been achieved. The revision also incorporates the various types of the materials currently being produced and consumed in the country. 0.4 In this revkic~: additional requirements for ash content, and for freedom from fish oil, linseed oil, blown oils and rosin have beenincluded. In place of four types in the original standard, the present revision prescribes eight types of the material and consequently the requirements for viscosity and acid value have also been suitably modified. The requirement for saponification value has been aligned with ISO/R 276. The test for viscosity has been adopted from BS 188 : 1957 `Determination of the viscosity of liquids in CGS units' issued by the British Standards Institution. The title of the standard has been suitably modified. 0.5 Thisstandard contains clause 5.1 which calls for agreement between the purchaser and the supplier. 0.6 For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS : 2-1960*. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard. *Rules for rounding off numerical values (mid). 3 IS I 79-1915 1. SCOPE 1.1 This standard prescribes requirements test for linseed stand oil for paints. 2. TERMINOLOGY 2.1 For the purpose of this standard, the definitions given in 2 of IS : 74- 1966* and IS : 1303- 1963t shall apply. 3. TYPES 3.1 There shall be eight types of the material as follows: a) b) c) d) Extra light, Light, Medium, Medium high, e) f) g) h) High, Extra high, Heavy, and Extra heavy. and methods of sampling and 4. REQVlREMENTS 4.1 Description - The material shall be polymerized linseed oil obtained only by heat treatment from linseed oil. It shall be free from sediment, insoluble matter and other oils. 4.2 Freedom from Fish and Linseed Oils the test when tested as prescribed in Appendix A. The material shall pass 1. 4.3 The material shall also conform to the requirements given in Table 5. PACKING AND MARKING 5.1 Packing - The material shall be supplied packed in suitable containers as agreed to between the purchaser and the supplier. 5.2 Markinga) b) c) d) e) The containers shall be marked with the following: Name and type of the material; Manufacturer's name or his recognized trade-mark, if any; Mass of the material; Batch number or lot number in code or otherwise; and Month and year of manufacture. *Methods of sampling and test for drying oils for paints (jrsf revision). tG1ossax-y of terms relating to paints (rekced). 4 TABLE 1 REQUIREMENTS FOR LINSEED STAND OIL FOR PAINTS (Clause 4.3) SL CZLkRACTERlSTlC No. rType 1 Type 2 (4) REQUIREMENT FOR L Type Ty TTY Type 3 6 (5) (6) (7) (8) METHOD OF TEST, REP TO Type 7 (9! TY$ (10) `----zGz Appendix IS : 74-1966' (1) i) Odour (2) (3) (11) (12) 5 9 10 12 19 3.5 & 5 23 ~----Similar 4-6 6 4 f 4 t-As < to that of the approved 70-75 18 sample-----t 90-100 20 200-250 22 + , + B & - ii) Viscosity at 3O"C, stokes iii) Acid value, Max 14-16 30-35 45-50 55-60 10 12 14 16 ur iv) Saponification value -186 to 200 2.0 0.10 agreed to between the supplier and the purchaserNegative v) Unsaponifiable matter, percent by mass, Max vi) Ash, percent by mass, Afax vii) Clarity and colour viii) Lieberman-starch-Morawski test for freedom from rosin (colophony) ix) Test for presence of blown oil c_--_---- Negative ----..-.- -+ C - t: .. G? I *Methods of sampling and test for drying oils for paints (Jirstrevti~n). IS : 79 - 1975 5.2.1 The Mark. containers may also be marked with the ISI Certification NOTE-The use of the IS1 Certification Mark is governed by the provisions of the Indian Standards Institution (Certification Marks) Act and the Rules and Regulations made thereunder. The IS1 Mark on products covered by an Indian Standard conveys the assurance that they have been produced to comply with the requirements of that standard under a well-defined system of inspection, testing and quality control which is devised and supervised by IS1 and operated by the producer. IS1 marked products are also continuously checked by IS1 for conformity to that standard as a further safeguard. Details of conditions under which a licence for the use of the IS1 Certification Mark may be granted to manufacturers or processors, may be obtained from the Indian Standards Institution. 6. SAMPLES 6.1 Representative of IS : 74-1966*. 7. TEST samples of material shall be drawn as prescribed under 3 METHODS 7.1 Tests shall be conducted as prescribed in IS : 74-1966* and Appendices A to C. References to relevant Appendices B and C and clauses of IS : 74-1966* are given in co1 11 and 12 of Table 1 respectively, and to Appendix A in 4.2. 7.2 Quality of Reagents-Unless specified otherwise, pure chemicals and distilled water (see IS : 1070-1960t) shall be employed in tests. NOTE - `Pure chemicals' shall mean chemicals that do not contain impurities which affect the results of analysis. 8. CRITERIA FOR CONFORMITY 8.1 A lot shall be declared as conforming to this standard if the test results of the composite sample satisfy the requirements prescribed under 4. APPENDIX (Clause 4.2) TEST FOR FREEDOM FROM A OILS FISH AND LINSEED A-O. GENERAL A-O.1 Outline of the Method - The addition of bromine to unsaturated fatty acids of fish oil in a petroleum hydrocarbon solvent gives a precipitate. The formation of a precipitate of hexabromide when the oil is treated with bromine in chloroform and then with alcohol and ether indicates the presence of linseed oil. *Methods of sampling and test for drying oils for paints (Jirsl rcvbion). tSpecification for water, distilled quality @vised). 6 IS : 79 - 1975 A-l. REAGENTS A-l .l Petroleum Hydrocarbon conformingto IS : 1745-l 966*. A-l .2 Bromine A-l .3 Chloroform A-l.4 Rectified Spirit conforming to IS : 323-1959t. Solvent 145/205 (low aromatic), A-l.5 Ether - conforming to solvent grade of IS : 336-1964:. A-2. PROCEDURE A-2.1 Test for Freedom from Fish Oil - Remove the moisture present, if any, by filteringthrough double layer filterpaper. Dissolve 2 to 3 ml of the sample in 20 ml of the petroleum hydrocarbon solvent in a test tube. Mix well and keep in a freezer maintained at 10 f 1°C for 5 minutes. Add broxnine drop by drop from a burette avoiding vigorous action until a considerable excess is present as indicated by the presence of a strong red colour. Shake well and allow to stand in cold water at a temperature of 25°C for 15 minutes. The material shall be taken to have passed this test if no cloudiness develops. A-2.1.1 If cloudiness or a precipitate appears due to bromination of the sample proceed as prescribed in A-2.1.1.1 to A-2.1.1.3. A-2.1.1.1 Saponify 2 to 3 ml of the sample in a IOO-ml Erlenmeyer flask adding 3 ~1, of sodium hydroxide solution (50 percent) and 3 ml of ethanol. Place the mixture on a steam-bath and heat for about an hour under reflux. Remove the condenser and remove the ethanol avoiding evaporation to dryness. Add 40 ml hot water and boil for an hour to remove the traces of the ethanol. Pour the mixture into a 250-ml separatory iinnel, washing the flask with 20 ml portions of boiling water. Acidify the mixture with 2 ml of 9 N sulphuric acid. Allow to settle until the fatty acids form a clear layer and the mixture is quite cold. Draw off the acid layer as completely as possible and wash the oil layer witk 20 ml portions of saturated sodium chloride solution. Reject the washings. Add 20 ml of diethyl ether and dissolve the fatty acids by gently swirling the separatory funnel. A-2.1.1.2 Transfer the solution in a test tube and cool to 10 & 1°C for 5 minutes. Add bromine drop by drop from a burette avoiding vigorous action until a considerable excess is present as indicated by the presence of a strong red colour. Shake well and allow to stand in cold water at a temperature of 25°C for 15 minutes. Centrifuge or filter and wash the precifiitate with *Specification tSpecification $Specification for petroleum hydrocarbon solvents for recified spirit (reui.5~~). for ether (re0ke~I). (retied). 7 IS : 79 - 1975 5 ml portions of ethyl ether. point of the precipitate. Dry to remove the ether. Check the melting A-2.1.1.3 The material shall be taken to have passed this test if the precipitate me!ts completely at 180 to 183"C, leaving no residue or blackening of the material. A-2.2 Test for Freedom from Linseed Oil - Pipette 1 ml of sample in a dry test tube which may be fitted with a ground glass stopper. Add 5 ml of chloroform and about 1 ml of bromine dropwise till the mixture is deep red in colour. Cool the test tube in ice water-bath. Add about 1.5 ml of rectified spirit in drops with shaking until the precipitate which is formed just dissolves and then add 10 ml of ether. Mix and place the tube in the ice-bath for 30 minutes. Appearance of a precipitate or cloudiness indicates the presence of linseed oil. A-2.2.1 The requirement of this test shall be taken to have been satisfied if no precipitate or cloudiness appears. APPENDIX [T&de 1, Item (ii)] DETERMINATION B-l. B-l.1 APPARATUS Fall Tube and Thermostat Bath B OF VISCOSITY B-1.1.1 The fall tube (see Fig. 1), shall be supported vertically in a bath, which shall be constructed of clear glass or shall have clear glass windows of such length as to allow observation of all graduations on the fall tube. The bath shall be filled to at least 3 cm above the topmost graduation of the fall tube. The bath shall be provided with a cover, bored to carry the thermometer and a tube to hold the balls to be used for the test. It shall be provided with means for efficient stirring and for convenient location of the fall tubes in a vertical position to within 1". The temperature of the bath shall be controlled by a thermostat so that the temperature variation in the bath is less than &-0.015"C. B-1.1.2 Fall tubes shall be constructed of clear glass free, as far as possible, from visible defects and to the design and dimensions shown in Fig. 1. The nominal internal diameter shall be not less than 10 times the diameter of the ball; 25 mm and 40 mm are suitable. Precision-bore tubing may be used. 8 Is : 79-1975 5 IO GLASS TUBE WITH FUNNEL TOP COVER OF BATH A- 220' t 200 25 175 I75 I ALTERNATIVES 100 1 75 I 25 - 25 t u 0 LO 60RE *See IS : 5165.1969 Specification for interchangeable in millimetres. conical 25 BORE ground-glass joints. All dimensions FIO. 1 FALLINCJ SPHERE VISCOMETER DIAGRAM OF FALL TUBE AND OF BALL-RELEASINO DEVICE WITH ALTERNATIVES 9 fS t 79-1975 B-1.1.3 The fall tubes shall be of overall length 320 & 3 mm; the lower end shall be rounded and the open end cut square to the axis. The tubes shall be etched with fine marks at distances as given in Fig. 1, measured from a line 30 mm distant from the closed end. These marks shall be carried right round the tube at right angles to the axis, and no interval shall be in error by more than 0.5 mm. The numbers shall be etched below the line in each case. To ensure axial delivery of the sphere, the fall tube shall be fitted either with a bored plug of inert non-absorbent material carrying a glass delivery tube or with a glass insert of the form shown in Fig. 1, adjusted so that the exit end of the tube will stand within 5 mm of the 220 mark on the fall tube. An internal diameter of 5 mm is suitable for use with a l/8-in ball designation, and of 2.5 mm with a l/16-in ball designation. It is assumed that steel balls will be used, but the procedure specified will be suitable for spheres made of other materials if they are no less truly spherical and their diameters and densities can be measured with the required accuracy. Steel balls may be obtained guaranteed to be within &O.OOO1 in of the nominal diameter (for a l/16-in ball this tolerance corresponds to an error of &0*3 percent in the viscosity). Steel balls shall be stored in liquid paraffin of IP quality or a similar preservative, to obviate rusting. Non-corroding steel balls are available. The rate of fall of the sphere depends on its size and the viscosity of the liquid under test. Table 2 indicates the approximate relationship of these factors. The values given are uncorrected for the restriction on rate of fall due to the walls of the tube. TABLE DESIGNATION OF STEEL SPHERE B-l .2 Sphere B-1.2.1 Selection of S'here - 2 BELATIONSHIP BETWEEN AND vI!.scoSITY BATE OF FALL I VISCOSITY OF LIQ7JmOF DENSITY0.8 g/cm' L Rate of Fall 1-O cm/s (2) cs 1 120 2 520 4490 7 010 Rate of Fall 0.3 cm/s (3) CS Rate of Fall 0.1 cm/s (4) cs Rate of Fall 0.03 cm/s (5) cs , (1) in l/16 3132 l/8 5132 NOTE 1 NOTE 2 - 3 740 l!E 23 400 11200 25 200 44 900 70 100 37 84 150 234 400 000 000 000 A rate of fall greater than 1 cm/s should NOTE 3shall be measured individually. A ball/tube diameter ratio greater than 1 : 10 should not be used. When balls smaller than l/16-in designation are selected their diameters not be used. 10 IS : 79 - 1975 B-1.2.2 Determination of the Density of the Sphere - This may be done by weighing a known number of balls after cleaning and drying. Makers of balls may be able to supply, from their own experience, information regarding the normal density and probable variation of their products. B-2. PROCEDURE B-2.1 Preparation of Sample - Filter the sample through a sintered glass filter or through a 75-micron sieve. Determine the density of the sample, at the temperature of test, by means of a density bottle or pyknometer. B-2.2 Filling the Fall Tube B-2.2.1 Fill the tube to at least 3 mm above the topmost mark with the filtered sample which has been brought approximately to the temperature of observation. It is essential that the sample be free from air bubbles, and care should be taken to avoid their formation, The tube shall be vertical. B-2.2.2 Leave the tube in the stirred bath for a sufficient time for air bubbles to clear and for temperature equilibrium to be attained. Usually a half to one hour is required when the filling temperature is near the test temperature. Longer times are necessary when the test and filling temperatures are markedly different. B-2.3 Determination of the Time of Fall B-2.3.1 Clean the sphere to remove grease, and immerse it in the sample under test, which is at a temperature with f 0.1% of the test temperature. Introduce it, without wiping, into the delivery tube by the aid of tweezers. B-2.3.2 By means of a reliable timing device, determine the time required for the sphere to fall through a suitable distance. The passage of the sphere may be observed by means of a telescope or other device for avoiding parallax error. The operation of the timing device is to coincide with the moments at which the lowest part of the sphere passes through the plane of the top of the timing marks. Normally the sphere is timed from the 175-mm mark to the 25-mm mark, but the time from the 200~mm mark to the O-mark may also be measured; if the fall is very slow, the definitive timing may be from the 175-mm mark to the loo-mm mark, using the time from the 200-mm mark to the 175-mm mark to provide a rough estimate of the rate. Obtain three readings agreeing within 0.5 percent. NOTE - Apart from inaccuracies of the timing device, using spheres of different density or size, or inefficient control of the temperature, failure to obtain good repeatability of results may be due to: (a) inhomogeneity ofthe liquid, caused, for example, by evaporation of the solvent from the surface+, or partial gelation and separation of invisible clots, etc; If the latter cause is suspected it is advisable to and (b) non-Newtonian behavtour. check the values obtained by using balls of different sizes and different portions of the tube. 11 IS : 79 - 1975 B-3. CALCULATIONS B-3.1 Calculate the kinematic following equations: viscosity V (centistokes) from one of the W-P) v= d2g0.181~~ x F where M= d= 6= P' V= g= mass in g of the sphere, diameter in cm of the sphere, density of the sphere in g/ems, density of the liquid in g/cm3, velocity of fall in cm/s, local acceleration due to gravity in cm/ss. F is known as the Faxen term and is a correction for the effect of wall of the fall tube on the motion of the sphere. If D is the diameter of the fall tube in cm, then the Faxen correction term is: F = 1 2.104 dlDs2.09 #/Ds--0.9 S/D6 _ For practical purposes, F is only required to the third place of decimals and the expression may be reduced to: F = 1.00 Some 2.104 d/D + 249 8/D" values of F are given in Table 3. TABLE 3 DESIGNATION OF SPHERE, d FAXEN CORRECTIONS I FAXEN CORRECTION, F c \ Internal Diameter of Tube D=25mm (1) in l/16 3132 l/8 5132 0.867 0.801 0.737 0.674 (2) I L D=4Omm (3) , 0.917 0.875 0.834 0.793 12 IS : 79 - 1975 l33.1.1 If a ball takes t seconds to fall 15 cm (that is, v = 15/t), in India (where g = 979.1 cm/s2), then equations (1) and (2) above may be reduced to: v = 692.3 Mt x d V = 362.6 d2t x If the nominal diameters are assumed for the balls, the equations become: V- KmMt x Some values in cgs units of Km and Kd, for a 150-mm sphere designations, are given in Table 4. TABLE DESXCNATION OF SPHERE I fall and for various 4 VALUES OF Km AND * K-d FOR 150-mm FALL IN t SECONDS D=25mm -zF---xxN2 D=40mm xc---Yz (3) (4) (5) , (1) in l/16 3132 l/8 5/32 (2) 3 791 2 335 1611 1 179 7.94 lG~51 27.00 38.58 4 009 2 550 1 823 1 387 8.40 18.03 30.55 45.39 APPENDIX C [Table 1, Item (ix)] TEST C-O. GENERAL C-O.1 Outline of the Method - Sample hydrocarbon solvent and examined. 13 is mixed with light petroleum FOR BLOWN OIL IS : 79 - 1975 c-l. El.1 joint. C-2. APPARATUS Measuring Cylinder - 50 ml capacity fitted with ground-glass REAGENT C-2.1 Petroleum Hydrocarbon conforming to IS : 1745; 1966*. C-3. PROCEDURE Solvent - boiling range 40 to 60°C C-3.1 Take 10 ml of the sample of linseed stand oil in a 50-ml measuring cylinder and mix it thoroughly with 30 ml of light petroleum hydrocarbon Observe the clarity of the solution once in the begmning and once solvent. after three days storage at room temperature. C-4. REPORT C-4.1 The sample shall be declared to have passed the test if the solution in initial observation is clear and it does not show any deposits after storage. *Specification for petroleum hydrocarbon solvents (retied). 14 BUREAU Heedquerters Telephones : OF INDIAN STANDARDS Manak Bhavan. 9 Bahadur Shah Zafar Marg. 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